CN110031444B - Raman spectrum measuring method under low temperature condition - Google Patents

Raman spectrum measuring method under low temperature condition Download PDF

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Publication number
CN110031444B
CN110031444B CN201910347059.0A CN201910347059A CN110031444B CN 110031444 B CN110031444 B CN 110031444B CN 201910347059 A CN201910347059 A CN 201910347059A CN 110031444 B CN110031444 B CN 110031444B
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optical fiber
fastener
optical
sample
optic fibre
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CN110031444A (en
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郭强
索奕双
张向平
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Jinhua Polytechnic
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Jinhua Polytechnic
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/10—Nuclear fusion reactors

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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention relates to the field of new material research and development, in particular to a Raman spectrum measuring method under a low-temperature condition, which is characterized in that a sample is placed in a sample chamber, and a fastener I and a fastener II of an optical feed-through are regulated so that the lower ends of a stainless steel tube and an optical fiber I are positioned at proper positions in the sample; in an experiment requiring real-time chemical reaction, introducing reaction gas into a sample chamber from an air inlet pipe, and reacting the reaction gas with a sample; the position of the optical fiber collimator is adjusted, so that laser emitted by the laser sequentially passes through the optical fiber III, the optical fiber coupler II, the optical fiber collimator, the plane mirror, the color separation filter and the optical fiber I and is incident to a sample, the wavelength of the laser is 532 nanometers, and the typical power value of the laser is 50 milliwatts; the Raman light generated in the sample sequentially passes through an optical fiber I, a color separation filter, a step filter, an optical fiber coupler I and an optical fiber II and enters a light detector; and transmitting the data of the Raman light acquired by the optical detector to a computer, and analyzing and processing the data by the computer to obtain corresponding information of the Raman light.

Description

Raman spectrum measuring method under low temperature condition
Technical Field
The invention relates to the field of new material research and development, in particular to a Raman spectrum measuring method under a low-temperature condition, which can carry out a Raman spectrum experiment under the low-temperature condition.
Background
The raman spectrum is a scattering spectrum, which is an analysis method for analyzing scattering spectrum different from the frequency of incident light to obtain information about vibration and rotation of molecules and applying the information to research on molecular structures, and some raman spectrum measurement experiments are required to be carried out under low temperature and vacuum conditions, so that an optical fiber is required to be introduced into a vacuum system, epoxy resin is usually adopted to seal between the optical fiber and a vacuum cavity in the prior art, a hollow conical teflon plug nested outside the optical fiber is inserted into a stainless steel tube and fastened by screws to achieve air tightness, the sealing method leads to excessive pressure on the optical fiber to lead to light attenuation and even lead to breakage of the optical fiber, and moreover, the teflon plug can be severely deformed after repeated use for a plurality of times, so that the sealing performance is reduced.
Disclosure of Invention
In order to solve the problems, the method of the invention adopts the vacuum feed-through with a special structure to introduce the optical fiber into the vacuum cavity so as to be suitable for direct optical fiber coupling in the low Wen Laman spectrum experiment, and can adjust the position of the optical fiber in situ, thereby prolonging the service life and reducing the fracture probability of the optical fiber on the basis of ensuring the air tightness.
The technical scheme adopted by the invention is as follows:
low temperatureThe Raman spectrum experimental device under the condition comprises a cooling cavity, a vacuum chamber, a sample, an optical fiber I, an optical feed-through, an air inlet pipe, an air outlet pipe, an optical cavity, a color separation filter, a step filter, an optical fiber coupler I, a plane mirror, an optical fiber collimator, an optical fiber coupler II, an optical fiber II, an optical detector, an optical fiber III, a laser, a cable and a computer, wherein xyz is a three-dimensional space coordinate system, the cooling cavity is provided with a low-temperature interlayer, the cooling cavity can be cooled by introducing low-temperature helium into the low-temperature interlayer, the experimental temperature ranges from 20K to 120K, the cooling cavity is provided with an operating arm, the vacuum chamber and the sample chamber are connected into the cooling cavity from top to bottom, the sample is positioned in the sample chamber, and an adsorption pump is arranged in the vacuum chamber, so that the lowest air pressure of vacuum asphyxia can reach 10 -4 The vacuum chamber is provided with a bottom through hole, flange edges are formed on the upper side and the lower side of the edge of the bottom through hole, the optical fiber I is provided with an optical fiber I protective layer and an optical fiber I core wire, the lower end of the optical fiber I is positioned in the sample chamber, the upper end of the optical fiber I is connected to the optical cavity, the color separation filter, the step filter, the optical fiber coupler I, the plane mirror, the optical fiber collimator, the optical fiber coupler II, the optical fiber II and the optical detector are all positioned in the vacuum chamber, the optical detector, the optical fiber II, the optical fiber coupler I, the step filter and the optical cavity are sequentially connected from top to bottom, the color separation filter is positioned in the optical cavity, the laser is positioned outside the cooling cavity, the laser, the optical fiber III, the optical fiber coupler II and the optical fiber collimator are sequentially connected from top to bottom, one end of the optical fiber collimator is fixed on the step filter, the position of the optical fiber coupler II can be changed through a micro-thread structure in the optical fiber collimator so as to adjust the position of a light spot of laser on a plane mirror, the plane mirror is positioned on the side of the optical cavity below the optical collimator, the optical fiber II, the optical fiber coupler II, the optical fiber II, the optical collimator II, the optical fiber collimator I, the optical fiber collimator I, the optical collimator I and the optical collimator I; the upper ends of the air inlet pipe and the air outlet pipe are positioned above the outside of the cooling cavity, and the lower ends of the air inlet pipe and the air outlet pipe penetrate through the vacuum chamber and are positioned in the sample chamber; the optical detector and the laser are connected with the computer by cables respectively, and the optical detector canThe collected optical information can be transmitted to a computer through a cable; the optical feed-through comprises a fastener I, a fastener II, a Teflon plug, a protective sleeve, a stainless steel tube, epoxy resin, a supporting gasket set and a small space, wherein the fastener I is hollow and provided with external threads, a conical opening is arranged below the fastener I, the fastener II is provided with internal threads, the bottom of the fastener II is provided with a through hole, the fastener I and the fastener II are respectively positioned on the upper side and the lower side of a bottom through hole of the vacuum chamber and are in threaded connection, the fastener I and the fastener II are respectively meshed with flange edges on the upper side and the lower side of the edge of the bottom through hole of the vacuum chamber, so that the fastener I and the fastener II are airtight with the bottom through hole of the vacuum chamber, the optical feed-through, the vacuum chamber and the cooling chamber are airtight, and the fastening degree of the fastener I and the fastener II can be adjusted through a cooling chamber manipulator arm; the Teflon plug comprises an upper hollow round table and a lower hollow cylinder, wherein the axis of the upper hollow round table and the axis of the lower hollow cylinder are integrally processed along the y direction, a through hole of the Teflon plug along the y direction is formed in the hollow part, the side surface of the round table is matched with a conical opening below a fastener I, the lower surface of the Teflon plug is in compression joint with the upper surface of a through hole at the bottom of a fastener II through a supporting gasket group, the supporting gasket group consists of two mutually overlapped and attached metal gaskets, the surfaces of the metal gaskets are polished, so that the friction resistance between the two metal gaskets is small, and when the Teflon plug rotates around a central shaft, the supporting gasket group can play a protection role on the Teflon plug so as to reduce the abrasion of the Teflon plug; in the fastening process of the fastening piece I and the fastening piece II, the fastening piece II applies force to the lower part of the Teflon plug through the supporting washer group, so that the Teflon plug is pressed upwards into the conical opening below the fastening piece I, a small space is formed among the fastening piece I, the fastening piece II and the Teflon plug, and fragments generated by abrasion of the Teflon plug can be accumulated in the small space; embedding a stainless steel tube into a fastener I, a Teflon plug and a fastener II from top to bottom, polishing the inner surface of the stainless steel tube, embedding an optical fiber I into the stainless steel tube, removing a part of an optical fiber I protective layer of the optical fiber I to expose an optical fiber I core wire with the length of 10 mm, wrapping the exposed optical fiber I core wire by adopting epoxy resin, embedding the optical fiber I into the stainless steel tube, and waiting forAfter the epoxy resin is solidified, the optical fiber I and the stainless steel tube can be fixed, the optical fiber I is provided with an epoxy resin wrapping section with the length of 10 mm and without an optical fiber I protective layer, the epoxy resin can bond and fix the core wire of the optical fiber I in the wrapping section with the inner surface of the stainless steel tube, the wrapping section is positioned in a fastener I above a Teflon plug in the fastener I, a protective sleeve is nested and fixed on the outer side of the stainless steel tube, and the protective sleeve is positioned at a position of 20 mm below the fastener II; the diameter of the through hole at the bottom of the fastener II is 4.8 mm; the radius of the upper bottom surface of the round table at the upper part of the Teflon plug is 4 mm, the radius of the lower bottom surface is 8.2 mm, the height is 6 mm, the radius of the cylindrical bottom surface at the lower part of the Teflon plug is 6 mm, the height is 5.2 mm, and the diameter of the through hole of the Teflon plug along the y direction is 3.8 mm; the inner diameter of the stainless steel tube is 0.6 mm, the outer diameter of the stainless steel tube is 3.6 mm, the tube wall of the stainless steel tube is thicker, and the transitional extrusion of the optical fiber I can be avoided; the inner diameter of the metal gasket of the supporting gasket set is 4 mm and the outer diameter is 12 mm.
The Raman spectrum measuring method under the low-temperature condition comprises the following steps:
step one, adjusting a fastener I and a fastener II of an optical feed-through an operating arm of a cooling cavity, so that the lower ends of a stainless steel tube and an optical fiber I are positioned at proper positions in a sample;
step two, introducing low-temperature helium into a low-temperature interlayer of the cooling cavity to cool the cooling cavity to 150K;
step three, starting an adsorption pump in the vacuum chamber to enable the vacuum in the vacuum chamber to reach 10 -4 The temperature of the cooling cavity is continuously reduced to 100K by Pascal;
step four, introducing reaction gas into a sample chamber from an air inlet pipe, and reacting the reaction gas with a sample;
step five, adjusting the position of the optical fiber collimator so that laser emitted by the laser sequentially passes through the optical fiber III, the optical fiber coupler II, the optical fiber collimator, the plane mirror, the color separation filter and the optical fiber I and is incident to a sample, wherein the wavelength of the laser is 532 nanometers, and the power of the laser is 50 milliwatts;
step six, raman light generated in the sample sequentially passes through an optical fiber I, a color separation filter, a step filter, an optical fiber coupler I and an optical fiber II and enters an optical detector;
and seventhly, transmitting the data of the Raman light acquired by the optical detector to a computer, and analyzing and processing the data by the computer to obtain corresponding information of the Raman light.
The beneficial effects of the invention are as follows:
the method adopts the specially designed vacuum feed-through and the novel optical fiber fixing method to introduce the optical fiber into the vacuum cavity, improves the service life of the vacuum feed-through and the optical fiber, reduces the risk of breakage of the optical fiber in the assembly process of introducing the optical fiber into the vacuum cavity, and has the function of in-situ adjusting the position of the optical fiber.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic illustration of the present invention;
fig. 2 is an enlarged partial schematic view of an optical feedthrough.
In the figure, 1, cooling chamber, 2, vacuum chamber, 3, sample chamber, 4, sample, 5-1, fiber I protective layer, 5-2, fiber I core, 6, optical feedthrough, 6-1, fastener I,6-2, fastener II,6-3, teflon plug, 6-4, protective sleeve, 6-5, stainless steel tube, 6-6, epoxy, 6-7, support gasket set, 6-8, small space, 7, air inlet tube, 8, air outlet tube, 9, optical chamber, 10, color separation filter, 11, step filter, 12, fiber coupler I,13, plane mirror, 14, fiber collimator, 15, fiber coupler II,16, fiber II,17, light detector, 18, fiber III,19.
Detailed Description
As shown in FIG. 1, the Raman spectrum experimental device under the low-temperature condition comprises a cooling cavity (1), a vacuum chamber (2), a sample chamber (3), a sample (4), an optical fiber I (5), an optical feed-through (6), an air inlet pipe (7), an air outlet pipe (8), an optical cavity (9), a color separation filter (10), a step filter (11), an optical fiber coupler I (12), a plane mirror (13), an optical fiber collimator (14), an optical fiber coupler II (15), an optical fiber II (16), an optical detector (17), an optical fiber III (18), a laser (19), a cable and a computer, wherein xyz is a three-dimensional space coordinate system, the cooling cavity (1) is provided with a low-temperature interlayer, and low-temperature helium gas is led into the low-temperature interlayer to enable the cooling cavityCan cool the cooling cavity (1), the experimental temperature ranges from 20K to 120K, the cooling cavity (1) is provided with a control arm, the vacuum chamber (2) and the sample chamber (3) are connected in the cooling cavity (1) from top to bottom, the sample (4) is positioned in the sample chamber (3), the adsorption pump is arranged in the vacuum chamber (2), and the lowest air pressure of the vacuum chamber (2) can reach 10 -4 The Pascal, vacuum chamber (2) has the bottom through-hole, the marginal upside and downside of bottom through-hole all have flange edge, optic fibre I (5) have optic fibre I protective layer (5-1) and optic fibre I heart yearn (5-2), the lower extreme of optic fibre I (5) is located sample room (3), the upper end is connected to optic cavity (9), colour separation filter (10), step filter (11), optic fibre coupler I (12), plane mirror (13), optic fibre collimator (14), optic fibre coupler II (15), optic fibre II (16) and light detector (17) all are located vacuum chamber (2), optic detector (17), optic fibre II (16), optic fibre coupler I (12), step filter (11) and optic cavity (9) are connected in proper order, colour separation filter (10) are located optic cavity (9), laser (19) are located outside cooling cavity (1), optic fibre III (18), optic fibre coupler II (15) and optic fibre collimator (14) are connected in proper order, the optic fibre II of collimator (14) is fixed in order on optic fibre (14) step filter's the inside of optic fibre (11), the little thread structure of optic fibre II can be changed from top to bottom, the position of a light spot of laser on a plane mirror (13) is adjusted, the plane mirror (13) is positioned on the side surface of an optical cavity (9) below an optical fiber collimator (14), an incident light path can be formed by a laser (19), an optical fiber III (18), an optical fiber coupler II (15), the optical fiber collimator (14), the plane mirror (13), a color separation filter (10) and an optical fiber I (5) in sequence, and a reflecting light path can be formed by a sample (4), the optical fiber I (5), the color separation filter (10), a step filter (11), the optical fiber coupler I (12), the optical fiber II (16) and a light detector (17) in sequence; the upper ends of the air inlet pipe (7) and the air outlet pipe (8) are positioned above the outside of the cooling cavity (1), and the lower ends of the air inlet pipe and the air outlet pipe penetrate through the vacuum chamber (2) and then are positioned in the sample chamber (3); the optical detector (17) and the laser (19) are respectively connected with the computer through cables, and the optical detector (17) can transmit the acquired optical information to the computer through the cables.
As shown in fig. 2, which is a partially enlarged schematic view of the optical feedthrough, the optical feedthrough (6) comprises a fastener I (6-1), a tight round piece II (6-2), a teflon plug (6-3), a protective sleeve (6-4), a stainless steel tube (6-5), an epoxy resin (6-6), a supporting gasket group (6-7) and a small space (6-8), wherein the fastener I (6-1) is hollow and provided with external threads, the lower surface of the fastener I (6-1) is provided with a conical opening, the fastener II (6-2) is provided with internal threads and the bottom is provided with a through hole, the fastener I (6-1) and the fastener II (6-2) are respectively positioned at the upper side and the lower side of the bottom through hole of the vacuum chamber (2) and are connected with threads, the fastener I (6-1) and the fastener II (6-2) are respectively meshed with flange edges of the upper side and the lower side of the bottom through hole of the vacuum chamber (2) so that the fastener I (6-1) and the fastener II (6-2) and the bottom through hole of the vacuum chamber (2) are provided with air tightness, the optical chamber (6), the optical chamber (2) and the cooling chamber (1) are provided with air tightness, the fastening degree of the fastening piece I (6-1) and the fastening piece II (6-2) can be adjusted through the control arm of the cooling cavity (1); the Teflon plug (6-3) comprises an upper hollow round table and a lower hollow cylinder, wherein the upper hollow round table and the lower hollow cylinder are integrally processed, the axes of the upper hollow round table and the lower hollow cylinder are in a y direction, a through hole of the Teflon plug (6-3) is formed in the hollow part, the side surface of the round table is matched with a conical opening below the fastener I (6-1), the lower surface of the Teflon plug (6-3) is in compression joint with the upper surface of a through hole at the bottom of the fastener II (6-2) through a supporting gasket group (6-7), the supporting gasket group (6-7) consists of two metal gaskets which are overlapped and attached with each other, the surfaces of the metal gaskets are polished, so that the friction resistance between the two metal gaskets is small, and when the Teflon plug (6-3) rotates around a central shaft, the supporting gasket group (6-7) can play a protection role in reducing the abrasion of the Teflon plug (6-3); during the fastening process of the fastening piece I (6-1) and the fastening piece II (6-2), the fastening piece II (6-2) applies force to the lower part of the Teflon plug (6-3) through the supporting washer group (6-7), so that the Teflon plug (6-3) is pressed upwards into the conical opening below the fastening piece I (6-1), a small space (6-8) is formed among the fastening piece I (6-1), the fastening piece II (6-2) and the Teflon plug (6-3), and fragments generated by abrasion of the Teflon plug (6-3) can be accumulated in the small space (6-8); the stainless steel tube (6-5) is nested into the fastening piece I (6-1), the Teflon plug (6-3) and the fastening piece II (6-2) from top to bottom, the inner surface of the stainless steel tube (6-5) is polished, the optical fiber I (5) is nested in the stainless steel tube (6-5), a part of the optical fiber I protective layer (5-1) of the optical fiber I (5) is removed, the optical fiber I core wire (5-2) with the length of 10 mm is exposed, the exposed optical fiber I core wire (5-2) is wrapped by adopting epoxy resin (6-6), the optical fiber I (5) is nested in the stainless steel tube (6-5), after the epoxy resin (6-6) is solidified, the optical fiber I (5) and the stainless steel tube (6-5) can be fixed, the epoxy resin (6-6) wrapping section with the optical fiber I protective layer (5-1) with the length of 10 mm can bond the optical fiber I core wire (5-2) in the wrapping section with the optical fiber I core wire (5-2) and the optical fiber I core wire (6-6) so that the optical fiber I is fixed on the surface of the fastening piece I (6-1) and the Teflon plug (6-1) is positioned in the fastening piece I (6-1), the outer side of the stainless steel pipe (6-5) is nested and fixed with a protective sleeve (6-4), and the protective sleeve (6-4) is positioned at a position 20 mm below the fastener II (6-2); the diameter of the through hole at the bottom of the fastener II (6-2) is 4.8 mm; the radius of the upper bottom surface of the round table at the upper part of the Teflon plug (6-3) is 4 mm, the radius of the lower bottom surface is 8.2 mm, the height is 6 mm, the radius of the cylinder bottom surface at the lower part of the Teflon plug (6-3) is 6 mm, the height is 5.2 mm, and the diameter of the through hole of the Teflon plug (6-3) along the y direction is 3.8 mm; the inner diameter of the stainless steel tube (6-5) is 0.6 mm, the outer diameter of the stainless steel tube is 3.6 mm, the tube wall of the stainless steel tube (6-5) is thicker, and the transitional extrusion of the optical fiber I (5) can be avoided; the inner diameter of the metal gasket of the supporting gasket set (6-7) is 4 mm, and the outer diameter is 12 mm.
The Raman spectrum experimental device under the low-temperature condition comprises a cooling cavity (1), a vacuum chamber (2), a sample chamber (3), a sample (4), an optical fiber I (5), an optical feed-through (6), an air inlet pipe (7), an air outlet pipe (8), an optical cavity (9), a color separation filter (10), a step filter (11), an optical fiber coupler I (12), a plane mirror (13), an optical fiber collimator (14), an optical fiber coupler II (15), an optical fiber II (16), a light detector (17), an optical fiber III (18), a laser (19), a cable and a computer, xyz is a three-dimensional space coordinate system, the cooling cavity (1) is provided with a low-temperature interlayer, the cooling cavity (1) can be cooled by introducing low-temperature helium gas into the low-temperature interlayer, the experimental temperature range is from 20K to 120K, the cooling cavity (1) is provided with a manipulator arm, the vacuum chamber (2) and the sample chamber (3) are connected into the cooling cavity (1) from top to bottom, the sample (4) is positioned in the sample chamber (3), and an adsorption pump is arranged in the vacuum chamber (2) so that the lowest air pressure of the vacuum chamber (2) can reach the lowest air pressure of the pressure 10 -4 The Pascal, vacuum chamber (2) has the bottom through-hole, the marginal upside and downside of bottom through-hole all have flange edge, optic fibre I (5) have optic fibre I protective layer (5-1) and optic fibre I heart yearn (5-2), the lower extreme of optic fibre I (5) is located sample room (3), the upper end is connected to optic cavity (9), colour separation filter (10), step filter (11), optic fibre coupler I (12), plane mirror (13), optic fibre collimator (14), optic fibre coupler II (15), optic fibre II (16) and light detector (17) all are located vacuum chamber (2), optic detector (17), optic fibre II (16), optic fibre coupler I (12), step filter (11) and optic cavity (9) are connected in proper order, colour separation filter (10) are located optic cavity (9), laser (19) are located outside cooling cavity (1), optic fibre III (18), optic fibre coupler II (15) and optic fibre collimator (14) are connected in proper order, the optic fibre II of collimator (14) is fixed in order on optic fibre (14) step filter's the inside of optic fibre (11), the little thread structure of optic fibre II can be changed from top to bottom, the position of a light spot of laser on a plane mirror (13) is adjusted, the plane mirror (13) is positioned on the side surface of an optical cavity (9) below an optical fiber collimator (14), an incident light path can be formed by a laser (19), an optical fiber III (18), an optical fiber coupler II (15), the optical fiber collimator (14), the plane mirror (13), a color separation filter (10) and an optical fiber I (5) in sequence, and a reflecting light path can be formed by a sample (4), the optical fiber I (5), the color separation filter (10), a step filter (11), the optical fiber coupler I (12), the optical fiber II (16) and a light detector (17) in sequence; the upper ends of the air inlet pipe (7) and the air outlet pipe (8) are positioned above the outside of the cooling cavity (1), and the lower ends of the air inlet pipe and the air outlet pipe penetrate through the vacuum chamber (2) and then are positioned in the sample chamber (3); the optical detector (17) and the laser (19) are respectively connected with the computer through cables, and the optical detector (17) can transmit the acquired optical information to the computer through the cables; the optical feed-through (6) comprises a fastener I (6-1), a fastener II (6-2), a Teflon plug (6-3), a protective sleeve (6-4), a stainless steel tube (6-5), epoxy resin (6-6), a supporting gasket group (6-7) and a small space (6-8), wherein the fastener I (6-1) is hollow and provided with external threads, the lower surface of the fastener I (6-1) is provided with a conical opening, the fastener II (6-2) is provided with internal threads and the bottom is provided with a through hole, and the fastener I (6-1) and the fastener II (6-2) are respectively positioned on the upper side and the lower side of the bottom through hole of the vacuum chamber (2)The side and thread connection is realized, the fastening piece I (6-1) and the fastening piece II (6-2) are respectively meshed with flange edges on the upper side and the lower side of the edge of the bottom through hole of the vacuum chamber (2), so that the tightness is formed between the fastening piece I (6-1) and the fastening piece II (6-2) and the bottom through hole of the vacuum chamber (2), the tightness is formed between the optical feed-through (6), the vacuum chamber (2) and the cooling chamber (1), and the fastening degree of the fastening piece I (6-1) and the fastening piece II (6-2) can be adjusted through the operating arm of the cooling chamber (1); the Teflon plug (6-3) comprises an upper hollow round table and a lower hollow cylinder, wherein the upper hollow round table and the lower hollow cylinder are integrally processed, the axes of the upper hollow round table and the lower hollow cylinder are in a y direction, a through hole of the Teflon plug (6-3) is formed in the hollow part, the side surface of the round table is matched with a conical opening below the fastener I (6-1), the lower surface of the Teflon plug (6-3) is in compression joint with the upper surface of a through hole at the bottom of the fastener II (6-2) through a supporting gasket group (6-7), the supporting gasket group (6-7) consists of two metal gaskets which are overlapped and attached with each other, the surfaces of the metal gaskets are polished, so that the friction resistance between the two metal gaskets is small, and when the Teflon plug (6-3) rotates around a central shaft, the supporting gasket group (6-7) can play a protection role in reducing the abrasion of the Teflon plug (6-3); during the fastening process of the fastening piece I (6-1) and the fastening piece II (6-2), the fastening piece II (6-2) applies force to the lower part of the Teflon plug (6-3) through the supporting washer group (6-7), so that the Teflon plug (6-3) is pressed upwards into the conical opening below the fastening piece I (6-1), a small space (6-8) is formed among the fastening piece I (6-1), the fastening piece II (6-2) and the Teflon plug (6-3), and fragments generated by abrasion of the Teflon plug (6-3) can be accumulated in the small space (6-8); the method comprises the steps of embedding a stainless steel pipe (6-5) into a fastener I (6-1), a Teflon plug (6-3) and a fastener II (6-2) from top to bottom, polishing the inner surface of the stainless steel pipe (6-5), embedding the optical fiber I (5) into the stainless steel pipe (6-5), removing part of an optical fiber I protective layer (5-1) of the optical fiber I (5) to expose an optical fiber I core wire (5-2) with the length of 10 mm, wrapping the exposed optical fiber I core wire (5-2) by epoxy resin (6-6), embedding the optical fiber I (5) into the stainless steel pipe (6-5), fixing the optical fiber I (5) and the stainless steel pipe (6-5) after the epoxy resin (6-6) is solidified, wrapping the optical fiber I (5) with an epoxy resin (6-6) with the length of 10 mm, wherein the epoxy resin is provided with the optical fiber I protective layer (5-1)(6-6) the core wire (5-2) of the optical fiber I in the wrapping section can be adhered and fixed with the inner surface of the stainless steel tube (6-5), the wrapping section is positioned in the fastener I (6-1) above the Teflon plug (6-3) in the fastener I (6-1), the outer side of the stainless steel tube (6-5) is nested and fixed with a protective sleeve (6-4), and the protective sleeve (6-4) is positioned at a position of 20 mm below the fastener II (6-2); the diameter of the through hole at the bottom of the fastener II (6-2) is 4.8 mm; the radius of the upper bottom surface of the round table at the upper part of the Teflon plug (6-3) is 4 mm, the radius of the lower bottom surface is 8.2 mm, the height is 6 mm, the radius of the cylinder bottom surface at the lower part of the Teflon plug (6-3) is 6 mm, the height is 5.2 mm, and the diameter of the through hole of the Teflon plug (6-3) along the y direction is 3.8 mm; the inner diameter of the stainless steel tube (6-5) is 0.6 mm, the outer diameter of the stainless steel tube is 3.6 mm, the tube wall of the stainless steel tube (6-5) is thicker, and the transitional extrusion of the optical fiber I (5) can be avoided; the inner diameter of the metal gasket of the supporting gasket set (6-7) is 4 mm, and the outer diameter is 12 mm.
The method for installing the optical feed-through (6) and the optical fiber I (5) comprises the following steps:
firstly, removing an optical fiber I protective layer (5-1) on the middle part of an optical fiber I (5), exposing an optical fiber I core wire (5-2) with the length of 10 mm, wrapping the exposed optical fiber I core wire (5-2) by adopting epoxy resin (6-6), embedding the optical fiber I (5) into a stainless steel tube (6-5), and fixing the optical fiber I (5) and the stainless steel tube (6-5) after the epoxy resin (6-6) is solidified;
secondly, arranging a fastener I (6-1) and a fastener II (6-2) on the upper side and the lower side of a bottom through hole of the vacuum chamber (2) respectively, arranging a Teflon plug (6-3) in a conical opening at the lower side of the fastener I (6-1), arranging a supporting washer group (6-7) in the fastener II (6-2), nesting the fastener I (6-1) in the bottom through hole of the vacuum chamber (2), and fixing the fastener I (6-2) through threads;
thirdly, the lower end of the stainless steel tube (6-5) is sequentially embedded into a fastener I (6-1), a Teflon plug (6-3), a supporting gasket group (6-7) and a fastener II (6-2), and the part of the optical fiber I (5) exposed out of the core wire (5-2) of the optical fiber I is positioned in the fastener I (6-1);
fourthly, nesting and fixing the protective sleeve (6-4) on the outer side of the lower end of the stainless steel tube (6-5);
fifthly, screwing the screw thread between the fastener I (6-1) and the fastener II (6-2) to ensure that the fastener I (6-1) and the fastener II (6-2) are airtight with the through hole at the bottom of the vacuum chamber (2), and applying a reverse torque to the protective sleeve (6-4) by a spanner to protect the optical fiber I (5) from being broken by the overlarge torque in the process of screwing the screw thread between the fastener I (6-1) and the fastener II (6-2);
the mode of operation and the principle of repeated use of the optical feed-through (6):
in the fastening process of the fastening piece I (6-1) and the fastening piece II (6-2), the fastening piece II (6-2) applies pressure to the lower surface of the Teflon plug (6-3) through the supporting gasket group (6-7), so that the Teflon plug (6-3) is pressed upwards into a conical opening at the lower side of the fastening piece I (6-1), a small cavity (6-8) is formed among the fastening piece I (6-1), the fastening piece II (6-2) and the Teflon plug (6-3), and fragments generated by abrasion of the Teflon plug (6-3) can be accumulated in the small space (6-8), thereby the elastic deformation of the Teflon plug (6-3) is not greatly influenced, the plastic deformation of the Teflon plug (6-3) can be compensated by adjusting the fastening degree between the fastening piece I (6-1) and the fastening piece II (6-2), and the Teflon plug (6-3) can be used repeatedly; in addition, in the installation process of the optical feed-through (6) and the optical fiber I (5), the Teflon plug (6-3) is subjected to the pressure of the inner wall of the conical opening at the lower side of the fastener I (6-1) and the pressure exerted by the fastener II (6-2) through the supporting gasket group (6-7), so that the Teflon plug (6-3) generates pressure on the outer wall of the stainless steel tube (6-5), and the transitional extrusion on the optical fiber I (5) can be avoided because the wall of the stainless steel tube (6-5) is thicker and the outer diameter and the inner diameter are larger; in conclusion, the optical feedthrough (6) and the optical fiber I (5) mounting method adopted by the invention can overcome the defect of softer material of the Teflon material, so that the Teflon material has good sealing property and service life.
The principle of in-situ adjustment of the position of the optical fiber I (5) is that the Teflon plug (6-3) has good elasticity and is less influenced by abrasion fragments due to the structure of the optical feed-through (6) adopted by the device, so that the pressure of the Teflon plug (6-3) on the outer wall of the stainless steel tube (6-5) is reduced by adjusting the fastening degree between the fastening piece I (6-1) and the fastening piece II (6-2), namely, the positions of the stainless steel tube (6-5) and the optical fiber I (5) can be adjusted in situ by moving along the axis or rotating around the axis, and the supporting gasket group (6-7) can protect the Teflon plug (6-3) in the rotating process so as to reduce the abrasion of the Teflon plug (6-3).
The Raman spectrum measuring method under the low-temperature condition comprises the following steps:
step one, adjusting a fastener I (6-1) and a fastener II (6-2) of an optical feed-through (6) through an operating arm of a cooling cavity (1) so that lower ends of a stainless steel tube (6-5) and an optical fiber I (5) are positioned at proper positions in a sample (4);
step two, introducing low-temperature helium into a low-temperature interlayer of the cooling cavity (1) to cool the cooling cavity (1) to 150K;
step three, starting an adsorption pump in the vacuum chamber (2) to enable the vacuum in the vacuum chamber (2) to reach 10 -4 The temperature of the cooling cavity (1) is continuously reduced to 100K by Pascal;
step four, introducing reaction gas into the sample chamber (3) from the gas inlet pipe (7), and reacting the reaction gas with the sample (4);
step five, adjusting the position of the optical fiber collimator (14) so that laser emitted by the laser (19) sequentially passes through the optical fiber III (18), the optical fiber coupler II (15), the optical fiber collimator (14), the plane mirror (13), the color separation filter (10) and the optical fiber I (5) and is incident to the sample (4), wherein the wavelength of the laser is 532 nanometers, and the power of the laser is 50 milliwatts;
step six, raman light generated in the sample (4) sequentially passes through an optical fiber I (5), a color separation filter (10), a step filter (11), an optical fiber coupler I (12) and an optical fiber II (16) and enters an optical detector (17);
and seventhly, transmitting the data of the Raman light acquired by the optical detector (17) to a computer, and analyzing and processing by the computer to obtain corresponding information of the Raman light.
The method of the invention adopts a novel optical fiber fixing method to introduce the optical fiber into the vacuum cavity, can reduce the extrusion and the twisting of the optical fiber in the assembly and the position adjustment process, and enables the optical fiber and the vacuum feed-through to be reused for a plurality of times.

Claims (1)

1. A Raman spectrum measuring method under a low-temperature condition comprises a cooling cavity (1), a vacuum chamber (2), a sample chamber (3), a sample (4), an optical fiber I (5), an optical feed-through (6), an air inlet pipe (7), an air outlet pipe (8), an optical cavity (9), a color separation filter (10), a step filter (11), an optical fiber coupler I (12), a plane mirror (13), an optical fiber collimator (14), an optical fiber coupler II (15), an optical fiber II (16), a light detector (17), an optical fiber III (18), a laser (19), a cable and a computer, wherein xyz is a three-dimensional space coordinate system, the cooling cavity (1) is provided with a low-temperature interlayer, the cooling cavity (1) can be cooled by introducing low-temperature helium gas into the low-temperature interlayer, the experimental temperature range is from 20K to 120K, the cooling cavity (1) is provided with a manipulator arm, the vacuum chamber (2) and the sample chamber (3) are connected into the cooling cavity (1) from top to bottom, the sample (4) is positioned in the sample chamber (3), and the vacuum chamber (2) is internally provided with an adsorption pump (10) so that the lowest air pressure of the vacuum chamber (2) can be reached -4 The Pascal, vacuum chamber (2) has the bottom through-hole, the marginal upside and downside of bottom through-hole all have flange edge, optic fibre I (5) have optic fibre I protective layer (5-1) and optic fibre I heart yearn (5-2), the lower extreme of optic fibre I (5) is located sample room (3), the upper end is connected to optic cavity (9), colour separation filter (10), step filter (11), optic fibre coupler I (12), plane mirror (13), optic fibre collimator (14), optic fibre coupler II (15), optic fibre II (16) and light detector (17) all are located vacuum chamber (2), optic detector (17), optic fibre II (16), optic fibre coupler I (12), step filter (11) and optic cavity (9) are connected in proper order, colour separation filter (10) are located optic cavity (9), laser (19) are located outside cooling cavity (1), optic fibre III (18), optic fibre coupler II (15) and optic fibre collimator (14) are connected in proper order, the optic fibre II of collimator (14) is fixed in order on optic fibre (14) step filter's the inside of optic fibre (11), the little thread structure of optic fibre II can be changed from top to bottom, the position of a light spot of laser on the plane mirror (13) is regulated, the plane mirror (13) is positioned on the side surface of the optical cavity (9) below the optical fiber collimator (14), and the laser (19), the optical fiber III (18), the optical fiber coupler II (15), the optical fiber collimator (14), the plane mirror (13) and the color separation and filtration can be sequentially carried outThe piece (10) and the optical fiber I (5) form an incident light path, and a reflecting light path can be formed by a sample (4), the optical fiber I (5), a color separation filter (10), a step filter (11), an optical fiber coupler I (12), an optical fiber II (16) and a light detector (17) in sequence; the upper ends of the air inlet pipe (7) and the air outlet pipe (8) are positioned above the outside of the cooling cavity (1), and the lower ends of the air inlet pipe and the air outlet pipe penetrate through the vacuum chamber (2) and then are positioned in the sample chamber (3); the optical detector (17) and the laser (19) are respectively connected with the computer through cables, and the optical detector (17) can transmit the acquired optical information to the computer through the cables; the optical feed-through (6) comprises a fastener I (6-1), a fastener II (6-2), a Teflon plug (6-3), a protective sleeve (6-4), a stainless steel tube (6-5), epoxy resin (6-6), a supporting gasket group (6-7) and a small space (6-8), wherein the fastener I (6-1) is hollow and provided with external threads, the lower surface of the fastener I (6-1) is provided with a conical opening, the fastener II (6-2) is provided with internal threads and a through hole at the bottom, the fastener I (6-1) and the fastener II (6-2) are respectively positioned at the upper side and the lower side of a bottom through hole of the vacuum chamber (2) and are in threaded connection, the fastener I (6-1) and the fastener II (6-2) are respectively meshed with flanges at the upper side and the lower side of the edge of the bottom through hole of the vacuum chamber (2), the optical feed-through (6), the fastener I (6-1) and the fastener II (6-2) are provided with air tightness between the bottom through holes of the vacuum chamber (2), the optical feed-through (6), the vacuum chamber (2) and the cooling chamber (1) are provided with air tightness, and the fastening degree of the fastener I and the fastener II (6-2) can be adjusted through the fastener I and the fastener II (6-2) through by the cooling chamber through; the Teflon plug (6-3) comprises an upper hollow round table and a lower hollow cylinder, wherein the upper hollow round table and the lower hollow cylinder are integrally processed, the axes of the upper hollow round table and the lower hollow cylinder are in a y direction, a through hole of the Teflon plug (6-3) is formed in the hollow part along the y direction, the side surface of the round table is matched with a conical opening below the fastening piece I (6-1), the lower surface of the Teflon plug (6-3) is pressed and connected onto a through hole at the bottom of the fastening piece II (6-2) through a supporting gasket group (6-7), the supporting gasket group (6-7) consists of two metal gaskets which are overlapped and attached with each other, the surface of the metal gasket is polished, and when the Teflon plug (6-3) rotates around a central shaft, the supporting gasket group (6-7) can reduce abrasion of the Teflon plug (6-3); during the fastening process of the fastening piece I (6-1) and the fastening piece II (6-2), the fastening piece II (6-2) applies force to the lower part of the Teflon plug (6-3) through the supporting washer group (6-7) so that the Teflon plug (6-3) is pressed upwards under the fastening piece I (6-1)And forms a small space (6-8) between the fastener I (6-1), the fastener II (6-2) and the Teflon plug (6-3), and debris generated by the Teflon plug (6-3) due to abrasion can be accumulated in the small space (6-8); the stainless steel tube (6-5) is nested into the fastener I (6-1), the Teflon plug (6-3) and the fastener II (6-2) from top to bottom, the inner surface of the stainless steel tube (6-5) is polished, the optical fiber I (5) is nested in the stainless steel tube (6-5), the optical fiber I (5) is provided with an epoxy resin (6-6) wrapping section with the length of 10 mm and without the optical fiber I protective layer (5-1), the epoxy resin (6-6) can bond and fix the optical fiber I core wire (5-2) in the wrapping section with the inner surface of the stainless steel tube (6-5), the wrapping section is positioned in the fastener I (6-1) above the Teflon plug (6-3) in the fastener I (6-1), a protective sleeve (6-4) is nested and fixed on the outer side of the stainless steel tube (6-5), and the protective sleeve (6-4) is positioned at 20 mm below the fastener II (6-2); the diameter of the through hole at the bottom of the fastener II (6-2) is 4.8 mm; the radius of the upper bottom surface of the round table at the upper part of the Teflon plug (6-3) is 4 mm, the radius of the lower bottom surface is 8.2 mm, the height is 6 mm, and the radius of the cylinder bottom surface at the lower part of the Teflon plug (6-3) is 6 mm, and the height is 5.2 mm; the diameter of the through hole of the Teflon plug (6-3) along the y direction is 3.8 mm; the inner diameter of the stainless steel tube (6-5) is 0.6 mm, and the outer diameter is 3.6 mm; the inner diameter of the metal gasket of the supporting gasket group (6-7) is 4 mm, the outer diameter is 12 mm,
the method is characterized in that: the Raman spectrum measuring method under the low-temperature condition comprises the following steps:
step one, adjusting a fastener I (6-1) and a fastener II (6-2) of an optical feed-through (6) through an operating arm of a cooling cavity (1) so that lower ends of a stainless steel tube (6-5) and an optical fiber I (5) are positioned at proper positions in a sample (4);
step two, introducing low-temperature helium into a low-temperature interlayer of the cooling cavity (1) to cool the cooling cavity (1) to 150K;
step three, starting an adsorption pump in the vacuum chamber (2) to enable the vacuum in the vacuum chamber (2) to reach 10 -4 The temperature of the cooling cavity (1) is continuously reduced to 100K by Pascal;
step four, introducing reaction gas into the sample chamber (3) from the gas inlet pipe (7), and reacting the reaction gas with the sample (4);
step five, adjusting the position of the optical fiber collimator (14) so that laser emitted by the laser (19) sequentially passes through the optical fiber III (18), the optical fiber coupler II (15), the optical fiber collimator (14), the plane mirror (13), the color separation filter (10) and the optical fiber I (5) and is incident to the sample (4), wherein the wavelength of the laser is 532 nanometers, and the power of the laser is 50 milliwatts;
step six, raman light generated in the sample (4) sequentially passes through an optical fiber I (5), a color separation filter (10), a step filter (11), an optical fiber coupler I (12) and an optical fiber II (16) and enters an optical detector (17);
and seventhly, transmitting the data of the Raman light acquired by the optical detector (17) to a computer, and analyzing and processing by the computer to obtain corresponding information of the Raman light.
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CN1584724A (en) * 2004-06-01 2005-02-23 中国科学院上海光学精密机械研究所 Porous optical fiber Raman sealed pool
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